Treatment of staple fiber



Patented Aug. 27, 1946 TREATMENT or STAPLE FIBER Harmon Howorth andLaurence C. Holt, Pearisburg, Va., assignors to Celanese Corporation ofAmerica, a corporation of Delaware No Drawing. Application November 7,1944, Serial No. 562,391

This invention relates to the treatment of textile materials and relatesmore particularly to an improved process for rendering staple fibermaterials having a basis of cellulose acetate or other organicderivative of cellulose more amenable to textile processing operations.

An object of this invention is to provide a novel process for thetreatment of cellulose acetate or other organic derivative of cellulosestaple fiber materials to render the same more amenable to textileoperation such as combing, carding and the like.

Another object of this invention is the provision of a novelconditioning treatment for cellulose acetate or other organicderivativeof cellulose staple fiber material whereby these staple fibermaterials may be subjected to textile processing operations without thedevelopment of any detrimental amount of static electricity.

A further object of this invention is the provision of a conditioningtreatment for staple fiber materials having a basis of cellulose acetateor other organic derivative of cellulose in which harsh treatment of thestaple fiber materials during the conditioning operation is avoided.

Still another object of this invention is the provision of acondiitoning process for staple fiber materials having a basis ofcellulose acetate or organic derivative of cellulose in which the amountof moisture placed on the treated fibers during the conditioning issubstantially reduced.

Yet another object of this invention is the production of staple fibermaterials having a basis of cellulose acetate or other'organicderivative of cellulose of improved hand.

Other objects of this invention will appear from the following detaileddescription.

In the treatment of staple fiber materials, having a basis of celluloseacetate or other organic derivative of cellulose, which are to be spuninto yarns, threads and the like, various liquid conditioning agents areusually applied to the fibers to impart the desired textile processingproperties thereto. To be satisfactorily processed, the staple fibermaterials must not only possess particular frictional qualities but theelectrical qualities must be such that the fibers generate the minimumamount of static electricity during combing, carding, spinning and likeoperations where the fibers are in constant frictional contact. Thepresence of static electricity on the fibers creates a substantialproblem since it not only causes the fibers to stick to the machinery,but it also causes them to resist adherence to each other duringspinning operations. This dif- 10 Claims (01. 117-56) ficulty isparticularly aggravated when the textile operations are conducted underconditions of low temperature and low humidity.

The finishing or conditioning agents heretofore employed have usuallybeen applied to the textile materials in the form of an aqueou emulsionafter the textile materials were reduced to the form of staple fibers.Excess emulsion was removed by passing the staple fibers through squeezerolls and the like, and after drying, the conditioned fibers were readyfor textile processing. Such methods of applying the conditioning agentrequire that the aqueous emulsions be formulated with great care andthat the squeeze roll pressure be maintained with great uniformity toinsure that the total amount of conditioning agent applied to the staplefiber is constant and uniform at all times. Variations in squeeze rollpressure and possible evaporation of water from the emulsion had tobeconsidered and compensated for when processing the staple fibers.Since these factors always rendered a carefully controlled applicationof the conditioning agent to the fibers highly uncertain, this method ofapplying conditioning agents to staple fiber material has not proved tobe entirely satisfactory for the production of staple fiber materials ofuniform textile processing characteristics. Furthermore; the aqueouemulsion method of applying the conditioning agents tends to give thestaple fibers a harsh and wiry hand.

We have now discovered a novel process wherein these and otherdisadvantages arising out of prior methods of conditioning staple fibertextile materials are avoided. In accordance with the process of ourinvention, we apply a selfscouring or self-emulsifying lubricating agentcomprising mineral oil to a continuous filament yarn, associate thelubricated filaments into a tow and then apply, directly thereto, aconcentrated, substantially non-aqueous sulfonated conditioning agentbefore severing the filaments into staple fiber lengths. Optimum resultsare achieved employing a conditioning agent comprising the reactionproduct of a mixture of a long chain higher fatty acid, vegetable oiland a mineral oil with oleum, having added thereto a penetrating agent,and neutralized with alkali and a hydroxyalkyl amine. The conditioningagent is preferably applied at an elevated tem- V perature. The treatedtow may then be crimped,

' if desired, severed to the desired staple fiber length by suitablecutting means, and then blown directly into a continuous drier whereitis dried V 3 to the desired. moisture from about to 6.5% by weight.

The yarns to be treated in accordance with this invention may be made ofor contain any suitable organic derivatives of cellulose such as organicesters of cellulose and cellulose ethers. Examples of organic esters ofcellulose are cellulose acetate, cellulose propionate and cellulosebutyrate, or mixed esters such as cellulose acetate-butyrate orcellulose acetate-propionate, while examples of cellulose ethers areethyl cellulose and benzyl cellulose.

In applying the lubricating agent to the filaments, we preferably placethe finish on the filaments directly as they pass from the bottom of thespinning cabinet, as by leading the filaments over a rotating wick whichis partly submerged 1n a vessel containing the mineral oil lubricant.From 0.25 to 3% of the lubricating agent may be applied to the yarns butwe have found that optimum results are obtained when about 0.7 5% basedon the weight of the filaments,

of the mineral oil lubricant is applied to the continuous runningfilaments.

A number of the lubricated filaments are then gathered to form a tow offrom 100 to 500 ends and of a denier of 25,000 to 100,000, and thesulfonated conditioning agent is then placed directly on the tow. Thefinishing agent may be ap- 'lied by spraying directly on to the tow orby feeding a controlled thin stream of the finish on to the tow. Themost desirable results are obtained when this finish is applied to thetow in amounts of 0.35 to 2% by weight and at a temperature above 40 C.and preferably, at 50C., or even higher. After the finish has beenapplied to the tow, the latter may then be crimped, if desired, by beingpassed through a series of serrated crimping rolls or uns-erratedrollers may be used to force. the yarn into a chamber in such a way thatback pressure causes crimping, or by any other suitable crimping means.A permanent crimp is thus placed in the filaments. The crimped tow isthen cut to accurately controlled uniform lengths by means of a suitablecutting device and the staple lengths of fiber are dried in a continuousdrier. In lieu of employing a continuous drier after the filaments aresevered, the conditioned tow may be passed over a series of heated cansand thus dried, before being severed into staple fiber lengths. Thedrying is most satisfactorily effected at temperatures of 65 toAlthoughby ourv novel process, the conditioning agent is not applieddirectly to each of the fibers, following the direct application of the.lubricating agent, our method of applying the finish is extremelyeffective in producing staple fiber ma,- terials which are eminentlysatisfactory with regard to their hand and to their textile processingqualities. When subjected to combing, carding, spinning and othertextile operations, the staple fibers may be processed in a smooth andeven manner with the development of little or no static electricity. 7

7 In order further to illustrate our invention but without being limitedthereto, the following example is given:

Example A 25% solution of cellulose acetate of an acetyl value of about54%, calculatedas acetic acid, in 95/5 acetone/water, is extrudedthrough a spinneret into an evaporativeatmosphere in a spin;- 'ningcabinet'to form-a 120 denier, 4'0filament content, which is usuallyyarn. The yarn is drawn from the base of the spinning cabinet and passedover a rotating wick partly submerged in a vessel containing alubrieating agent comprising mineral oil and containing emulsifyingagents which render the lubri-. cant self-scouring when the yarn isimmersed in water. The contact between the yarn and the rotated wick isso adjusted that 0.75%, based on the weight of the yarn, of thelubricating agent is applied to the yarn. A number of yarns, with themineral oil finish contained thereon, are gathered together to form atow containing 30 ends of 36,000 total denier and passed through a pairof rolls which forces the yarns into a crimping chamber. 'Just prior toentering the crimping rolls which force the yarn into the crimp ingchamber, a controlled stream of the sulfonated conditioning agent,heated to 0., is fed on to the moving tow. The rate of feed is such asto place about 0.45% by weightof the finish on the tow. Back pressure inthe chamber places a permanent crimp in the yarns. The crimped tow isdrawn from the chamber and is then cut hand, and, due to their excellentanti-static -quality, may be processed with the production of a minimumamount of fly.

The mineral oil lubricating composition employed for the initialtreatment comprises mineral oil of about 50 to 100 Saybolt viscosity,together with small quantities of a sulfonated vegetable oil such assulfonated olive oil, peanut oil, rice oil or even sunflower oil,unsulfonated vegetable oil, oleic'acid, soap and water in amounts togive the desired'viscosity, stability and emulsification. The mineraloil may comprise about a by weight of the composition, which may containfrom 8 to 10% of sulfonated vegetable oil, about 3 to 4% of oleic acid,about 7 to 8% of unsulfonated vegetable oil, about 2% of a soap such assodium oleate, and 1% of water. The soap and sulfonated vegetable oilpresent render the lubricating composition self-emulsifying so that itmaybe scoured easily and completely from the staple fiber'm-aterialsafter they have been spun into yarns.

The sulfonated conditioning agent employed in accordance with theprocess of our invention is prepared by first reacting a mixture ofoleic acid, a vegetable oil such'as peanut oil, and mineral oil with 20%oleum whereby the oleic acid and vegetable oil are-partially sulfatedand/or sul fonated, and then addingto the sulfonated mixture a'spreading'and penetrating agent, such as diamyl phenol. Triethanolamineand aqueous sodium hydroxide are then added so as to substantiallyneutralize any free acid presentforming the sodium andtriethanolamine-sal-ts thereof. A fungicide such as sodium orthophenylphenate may also be added to inhibit the growth of any undesirableorganisms in the resulting mixture The preparation of such conditioningagents is t more particularly described in co-pendi-ng United Statesapplication S. No. 470,662filed on Decem ber 30, 1942.

Our novel method of applying the lubricant at the metier or spinningcabinet in the manner described and the application of the sulfonatedconditioning agent directly to the tow just prior to the crimping feedrolls permits extremely accurate control of the application of thelubricating and conditioning agents. The usual method of applying theconditioning agent in the form of an aqueous emulsion may thus beeliminated entirely and substantially improved staple fibers obtained.

Our novel method not only permits the finish to be applied accurately incarefully controlled amount, but it also eliminates the necessity forputting the staple fiber through harsh treatments during theconditioning treatment since squeeze rolls for removing excess emulsionand pin-strippers for breaking the matof fibers are no longer necessary.Also, the harsh opening treatment for opening the matted staple fiberpreviously necessary when the finishing agent was applied in emulsionform is avoided. Furthermore, as previously pointed out, the use ofsubstantially nonaqueous conditioning agent makes possible a substantialheat saving in the drying of the conditioned staple fibers since farless moisture must be removed to reduce the moisture content to thedesired degree. The elimination of the treatment of the staple fiberwith conditioning agents after the cutting operation also results in aconsiderable' saving in'space since additional equipment for thetreatment of the bulky staple fiber is no longer necessary.

It is to be understood that the foregoing detailed description is givenmerely by way of illustration and that many variations may be madetherein without departing from the spirit of our invention.

Having described our invention, what we desire to secure by LettersPatent is:

1. In a process for the production of staple fiber textile materials,having a basis of filaments of an organic derivative of cellulose, ofimproved textile processing characteristics, the step which comprisesapplying to a mineral oil lubricated, continuous filament textilematerial a substantially non-aqueous conditioning agent comprising theproduct formed by reacting a mixture of a mineral oil, a vegetable oil,a higher fatty acid and oleum at a temperature no greater than about 20C. whereby sulphonation of at least part of the higher fatty acid andvegetable oil occurs, to which product is added a spreading andpenetrating agent and an amount of alkali-metal hydroxide and analkylolamine to neutralize all of the oleum and the major portion of thehigher fatty acid. l 2. Ina process for the production of staple fibertextile materials, having a basis of filaments of an organic derivativeof cellulose, of improved textile processing characteristics, the stepwhich comprises applying to a mineral oil lubricated, continuousfilament textile material a substantially non-aqueous conditioning agentcomprising the product formed by reacting a mixture of a mineral oil, avegetable oil, a higher fatty acid and oleum at a temperature no greaterthan about 20 C. whereby sulphonation of at least part of the higherfatty acid and vegetable oil occurs, to which roduct is added analkylated phenol and an amount of alkali-metal hydroxide and analkylolamine to neutralize all of the oleum and the major portion of thehigher fatty acid.

3. In a process for the production of staple fiber textile materials,having a basis of filaments of an organic derivative of cellulose, ofimproved textile processing characteristics, the step which comprisesapplying to a mineral oil lubricated,

part of the higher fatty acid and vegetable oil occurs, to which productis added diamyl phenol and an amount of alkali-metal hydroxide and analkylolamine to neutralize all of the oleum and the major portion of thehigher fatty acid.

4. In a process for the production of staple fiber textile materials,having a basis of filaments of an organic derivative of cellulose, ofimproved textile processing characteristics, the step which comprisesapplying to amineral oil lubricated, continuous filament textilematerial a substantially non-aqueous conditioning agent comprising theproduct formed by reacting a mixture of a mineral oil, a vegetable oil,ahigher fatty acid and oleum at a temperature no greater than about 200. whereby sulphonation of at least part of the higher fatty acid andvegetable oil occurs, to which product is added an acetylated castor oiland'an amount of alkali-metal hydroxide and an alkylolamine toneutralize all of the oleum and the major portion of the highercomprises applying to a mineral oil lubricated,

continuous filament textile material a substantially non-aqueousconditioning agent comprising the product formed by reacting a mixtureof a mineral oil, a vegetable oil, oleic acid and oleum at a temperatureno greater than about 20% C. whereby sulphonation of at least part ofthe higher fatty acid and vegetable oil occurs, to which product isadded a spreading and penetrating agent and an amount of alkali-metalhydroxide and an alkylolamine to neutralize all of the oleum and themajor portion of the higher fatty acid.

6. In a process for the production of staple fiber textile materials,having a basis of filaments of an organic derivative of cellulose, ofimproved textile processing characteristics, they step which comprisesapplying to a mineral oil lubricated, continuous filament textilematerial a substantially non-aqueous conditioning agentcomprising theproduct formed by reacting a mixture of a mineral oil, a vegetable oil,oleic acid and oleum at a temperature no greater than about 20 C.whereby sulphonation of at least part of the higher fatty acid andvegetable oil occurs, to which product is added diamyl phenol and anamount of alkali-metal hydroxide and an alkylolamine to neutralize allof the oleum and the major portion of the higher fatty acid.

7. In a process for the production of staple fiber textile materials,having a basis of filaments of an organic derivative of cellulose, ofimproved textile processing characteristics, the step which comprisesapplying to a mineral oil lubricated, continuous filament textilematerial a substantially non-aqueous conditioning agent comprising theproduct formed by reacting a mixtureof mineral oil, raw peanut oil,oleic acid and oleum at a temperature no greater than about 20 C.whereby sulphonation of at least part of the higher fatty acid andvegetable oil occurs, to which product is added diamyl phenol and anamount of alkali-metal hydroxide and an alin tow form a substan iallynom queous -r tioning a ent comprisin the pr du t formed y reactin amixture of' mineral oil, a vegetable oil, a hi her fa ty acid and o e ma a temp rature no greater than about 20? C, wherebysulphonation of atleast part of the higher fatty acid and vegetable oil occurs, to whichproduct is added a spreading and penetrating agent and an amount ofalkali-metal hydro id and an kylolamine to neutralize all of the oleumand the major portion of the higher fatty acid.

9.'In a process for the production of staple fiber textile materia h vina. sis o fil ment of cellulose acetate, of improved textile processingcharacteristics, the step which comprises applying toa mineral oillubricated, continuous l filament textile material in tow form asubstantially honq s nditionin a nt ompri ing the product formed byreacting a mixture of a mineral oil, a, vegetable oil, a higher fattyacid 7 3 c and oleum at a temperat re no greater than about 20 C,whereby sulphonation of at least art of the higher fatty acid andVegetable oil o eours, to Which product is added a spreading andpenetrating agent and an, amount of alkali metal hydroxide and an a kyneto e tralize all of the oleum and the major portion of the higherfatty acid. 7

10. In a process for the production of Staple fiber textile materials,having a basis of fila ments of cellulose acetate of improved textileprocessing characteristics, the step which comprises applying at atemperature of at least 40 C to a mineral oillubricated,continuous filament textile material in tow form a substantially non-aqueousconditioning agent comprising the product formed by reacting a mixtureofa mineral oil, raw peanut oiLoleic acid and oleum at a temperature nogreater than about 20 C.

whereby sulphonation of at least part of the higher fatty acid andvegetable oil occurs, to

which product is added diamyl phenol and an amount of alkali-metalhydroxide and an al.- kylolamine to neutralize all of the oleum and themajor portion of the higher fatty acid.

HARMON HOWORTH. LAURENCE C. HOLT;

